March 26 2012: Conference ISIS 16h30, Prof. Lyndon EMSLEY, “Surface Enhanced NMR Spectrosopy”, ENS-Lyon (France)
Abstract: We have shown over the last few years that multi-dimensional magic-angle-spinning solid-state NMR spectroscopy can play a major role in characterizing a range of difficult materials, from macromolecules to polymorphs to catalysts. An overview of this progress will be given. In particular, sensitivity is a key problem in NMR, and we will demonstrate different approaches to increasing sensitivity. For example, we will show how surface NMR spectra can be greatly enhanced using DNP. Polarization is transferred from the protons of the solvent to the rare nuclei (at natural isotopic abundance) at the surface, yielding at up to a hundred-fold signal enhancement for surface species in silica frameworks. As examples of this approach, we demonstrate the fast characterization of the distribution of surface bonding modes and interactions in a series of functionalized materials using this technique. Surface enhanced carbon-13, silicon-29, nitrogen-15 and aluminum-27 DNP NMR spectra were obtained by using incipient wetness impregnation of samples with a solution containing a polarizing radical. Furthermore, the remarkable gain in time provided by surface enhanced DNP NMR spectroscopy (up to a factor 10 000) allows the facile acquisition of two-dimensional correlation spectra, allowing access to conformational features of the surface groups